CN102719060B - High-temperature resistant and high-gloss PET / PBT composite material and preparation method thereof - Google Patents
High-temperature resistant and high-gloss PET / PBT composite material and preparation method thereof Download PDFInfo
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a high-temperature and high-gloss PET / PBT composite material and a preparation method thereof. The PET / PBT composite is comprised of, by weight,100 parts of PET, 20-40 parts of PBT, 10-40 parts of a mineral filler, 3-10 parts of a flexibilizer, 0.3-0.6 part of an antioxidant, 0.2-0.6 part of a processing agent, 0.5-1.2 part of a heat-resistant agent and 0.5-1 part of a nucleating agent. The high-temperature and high-gloss PET / PBT composite material prepared by the present invention has the advantages of PET and PBT, and excellent forming and processing performance, suits for all kinds of complex structures, reduces the transesterification and improves temperature resistance of the material.
Description
[technical field]
The present invention relates to polymeric material field, relate in particular to a kind of high-temperature resistant high gloss PET/PBT matrix material and preparation method thereof.
[background technology]
PET(Polyethylene terephthalate, polyethylene terephthalate) be that a kind of degree of crystallinity is high, the vibrin of physics, chemical property excellence.Its material modified its has good mechanical property in wide temperature range, life-time service temperature can reach 140 ℃, electrical insulating property is good, even under high-temperature high-frequency, its electrical property, mechanical property are still better, rub resistance, dimensional stability is excellent, heat-drawn wire is high, but its corona resistance is poor, crystallization velocity is slow, resistance to low temperature is poor.PBT (Polybutylene terephthalate, polybutylene terephthalate) is the linear saturated polyester resin of a kind of crystal type, and its crystallization velocity is fast, can high-speed molding; Weathering resistance, electrical property, flame retardant properties, chemical proofing, friction wear excellent, water-absorbent is low, heat-drawn wire is high; Mechanical property is good, and physical strength is high, resistance to fatigue and good stability of the dimension, and creep is also less, these performances also changes little under hot conditions.
If can prepare the matrix material of PET and PBT, can make matrix material possess the advantage of PET and PBT simultaneously.
[summary of the invention]
The invention provides a kind of high-temperature resistant high gloss PET/PBT matrix material and preparation method thereof, this PET/PBT matrix material possesses the advantage of PET and PBT, and moulding processability excellence is applicable to all kinds of complex constructions, has reduced transesterify, improves the heat resistance of material.
Technical scheme of the present invention is:
A kind of high-temperature resistant high gloss PET/PBT matrix material, by weight, composed of the following components:
A preparation method for high-temperature resistant high gloss PET/PBT matrix material as described above, comprises the following steps:
Step 1, take each component by parts by weight described above;
Step 2, by each component taking through high-speed mixing process 10-15 minute;
Step 3, by mixed step 2 material, melt extrude granulation through twin screw extruder; Twin screw extruder processing condition are: district's temperature is 190-230 ℃, and two district's temperature are 220-250 ℃, and three district's temperature are 230-265 ℃, four district's temperature are 225-260 ℃, five district 230-265 ℃, compound time of delivery in screw rod is 1-5min, pressure is 10-18MPa.
High-temperature resistant high gloss PET/PBT matrix material prepared by the present invention, possesses the advantage of PET and PBT, and moulding processability excellence is applicable to all kinds of complex constructions, has reduced transesterify, improves the heat resistance of material.
[accompanying drawing explanation]
Accompanying drawing 1 is composite material test DSC figure prepared by the embodiment of the present invention 3.
Accompanying drawing 2 is composite material test DSC figure prepared by comparative example 2.
Accompanying drawing 3 is composite material test DSC figure prepared by comparative example 1.
[embodiment]
In order to make technical scheme of the present invention and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
High-temperature resistant high gloss PET/PBT matrix material of the present invention, by weight, is made up of following component:
Wherein, the function of PET is as major ingredient, aspect physical strength and heatproof, rise leading primary.The function of PBT is as auxiliary bed material, has auxiliaring effect to improving material injection moulding effect and mobility.The function of mineral-filled thing is the mechanical property that increases material, improves the heat-resisting of material, anti-warpage ability, the glossiness of raising material surface.The function of toughner is the toughness that increases material, promotes the toughness of material under cold condition.The function of oxidation inhibitor is to reduce the oxidation of material in process engineering.The function of processing aid is to reduce between material and material and the friction of material and equipment product, is convenient to processing, makes to fill to be evenly distributed.The function of heat-resistant agent is to reduce the transesterify of PET and PBT, improves resistance toheat.The function of nucleator is to improve and improve crystallization effect and the crystallization velocity of PET, improves the resistance toheat of material.
In following each specific embodiment, the preferred relative density of PET is 1.35-1.38g/cm3, and fusing point is 250-260 ℃, and its kinetic viscosity under molten state is 0.65-1.2 handkerchief second, mainly selects spinning grade polyester section; The preferred relative density of PBT is 1.30-1.34 g/cm3, and fusing point is 222-227 ℃, and its kinetic viscosity under molten state is 0.85-1.2 handkerchief second, if the place of production is Changchun, Taiwan, Mitsubishi or U.S. GE; The concrete preparation method of mineral-filled thing is as follows: silicates composite reinforcing fiber whisker, needle-like ground silica and process white are mixed by weight 1:0.5-0.6:0.5-0.6, separately add the nano silicon and the silane coupling agent that account for base-material gross weight 0.5%-2%, mix through high mixer, mixing temperature remains on 95 ℃, and mixing time is 30min; Wherein, silicates whisker is the silicate whisker of commercially available general aluminium class or calcium class, needle-like ground silica is commercially available 5000 general order needle-like ground silicas, particle diameter is between 2.5 um-3.4 um, process white is commercially available universal process white, and the model of silane coupling agent is KH550 or KH560; The preferred EPDM grafted maleic anhydride of toughner or acrylate connect the one in an Ethylene Propylene Terpolymer elastomerics, as the PTW of Du Pont, and PC-15 or KT-22; Antioxidant is four [3-(3 preferably, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and tricresyl phosphite (2,4-di-t-butyl phenyl ester) composite mixture or triglycol two-3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propylene dragonfly, three (2,4-di-tert-butylphenol) one (commercially available model PW-9225 in phosphorous acid ester, 1010,168,1076 etc.); One (commercially available model is Ke Laien OP wax, TAF, EBS) in the modified product of the preferred OP wax of processing aid, stearic acid class or fatty acid or ethylene bis stearamide; Heat-resistant agent preferably phosphoric acid triphenylmethyl methacrylate, Sodium Acid Pyrophosphate, ethyl sulfate, one or several mixture (with chemical pure cost performance the best) of the organic phosphoric acid compounds such as di (isooctyl) phosphate; Nucleator is preferably mixed by one or several in long-chain line style saturated carboxylic acid sodium salt, long-chain line style saturated carboxylic acid calcium salt and aromatic carboxylic acid metal sodium salt or magnesium salts.
Embodiment 1
In this embodiment, high-temperature resistant high gloss PET/PBT matrix material of the present invention, made by the raw material of following portions by weight:
100 parts of PET, 20 parts of PBT, 10 parts of mineral-filled things, 3 parts of toughner, 0.3 part, oxidation inhibitor, 0.2 part of processing aid, 0.5 part of heat-resistant agent, 0.5 part of nucleator.
Its preparation method is as follows:
Take by weight above-mentioned raw materials, in hasten stirrer for mixing 10 minutes of height, then extrude granulation through twin screw extruder.Wherein each zone temperatures is: district's temperature is 190 ℃, and two district's temperature are 220 ℃, and three district's temperature are 260 ℃, and four district's temperature are 255 ℃, five 265 ℃, districts, and compound time of delivery in screw rod is 3 minutes, pressure is 15MPa.
Embodiment 2
In this embodiment, high-temperature resistant high gloss PET/PBT matrix material of the present invention, made by the raw material of following portions by weight:
100 parts of PET, 28 parts of PBT, 20 parts of mineral-filled things, 5 parts of toughner, 0.4 part, oxidation inhibitor, 0.3 part of processing aid, 0.7 part of heat-resistant agent, 0.6 part of nucleator.
Its preparation method is as follows:
Take by weight above-mentioned raw materials, in hasten stirrer for mixing 12 minutes of height, then extrude granulation through twin screw extruder.Wherein each zone temperatures is: district's temperature is 210 ℃, and two district's temperature are 230 ℃, and three district's temperature are 250 ℃, and four district's temperature are 245 ℃, five 260 ℃, districts, and compound time of delivery in screw rod is 5 minutes, pressure is 18MPa.
Embodiment 3
In this embodiment, high-temperature resistant high gloss PET/PBT matrix material of the present invention, made by the raw material of following portions by weight:
100 parts of PET, 35 parts of PBT, 30 parts of mineral-filled things, 7 parts of toughner, 0.5 part, oxidation inhibitor, 0.5 part of processing aid, 1.0 parts of heat-resistant agents, 0.8 part of nucleator.
Its preparation method is as follows:
Take by weight above-mentioned raw materials, in hasten stirrer for mixing 15 minutes of height, then extrude granulation through twin screw extruder.Wherein each zone temperatures is: district's temperature is 190 ℃, and two district's temperature are 220 ℃, and three district's temperature are 260 ℃, and four district's temperature are 255 ℃, five 265 ℃, districts, and compound time of delivery in screw rod is 2 minutes, pressure is 15MPa.
Embodiment 4
In this embodiment, high-temperature resistant high gloss PET/PBT matrix material of the present invention, made by the raw material of following portions by weight:
100 parts of PET, 40 parts of PBT, 40 parts of mineral-filled things, 10 parts of toughner, 0.6 part, oxidation inhibitor, 0.6 part of processing aid, 1.2 parts of heat-resistant agents, 1 part of nucleator.
Its preparation method is as follows:
Take by weight above-mentioned raw materials, in hasten stirrer for mixing 10 minutes of height, then extrude granulation through twin screw extruder.Wherein each zone temperatures is: district's temperature is 220 ℃, and two district's temperature are 220 ℃, and three district's temperature are 260 ℃, and four district's temperature are 255 ℃, five 265 ℃, districts, and compound time of delivery in screw rod is 5 minutes, pressure is 12MPa.
Comparative example 1
High-temperature resistant high gloss PET/PBT matrix material of this comparative example, made by the raw material of following portions by weight:
100 parts of PET, 35 parts of PBT, 30 parts of mineral-filled things (without the mixed packing of special processing), 7 parts of toughner, 0.5 part, oxidation inhibitor, 0.5 part of processing aid.
Its preparation method is as follows:
Take by weight above-mentioned raw materials, in hasten stirrer for mixing 10 minutes of height, then extrude granulation through twin screw extruder.Wherein each zone temperatures is: district's temperature is 190 ℃, and two district's temperature are 220 ℃, and three district's temperature are 260 ℃, and four district's temperature are 255 ℃, five 265 ℃, districts, and compound time of delivery in screw rod is 3 minutes, pressure is 15MPa.
Comparative example 2
High-temperature resistant high gloss PET/PBT matrix material of this comparative example, made by the raw material of following portions by weight:
100 parts of PET, 35 parts of PBT, 30 parts of mineral-filled things, 7 parts of toughner, 0.5 part, oxidation inhibitor, 0.5 part of processing aid, 0.8 part of nucleator.
Its preparation method is identical with comparative example 1.
Performance test and evaluation:
By the particle material of above-described embodiment 1-4 and comparative example 1,2 preparations in air dry oven 110-120 ℃ dry 4 hours, and then dried particulate material is carried out in injector to injection molding sample preparation, injection mold temperature control is at 100 ℃.Testing residing room temperature environment is 23 ℃.
Wherein, tensile strength is tested by ISO 527 standards.Specimen types is I type, batten size (mm): 150 (length) × (20 ± 0.2) (end width) × (4 ± 0.2) (thickness), and draw speed is 50 mm/min;
Flexural strength and modulus in flexure are tested by ISO 178 standards.Specimen types is specimen size (mm): (80 ± 2) × (10 ± 0.2) × (4 ± 0.2), and rate of bending is 20 mm/min;
Notched Izod impact strength is tested by ISO 180 standards.Specimen types is I type, specimen size (mm): (80 ± 2) × (10 ± 0.2) × (4 ± 0.2); Breach type is category-A, and breach is thick 1/3 deeply;
Heat-drawn wire is tested by ISO 75-2 standard.Specimen types is I type, specimen size (mm): 127 (length) × (13 ± 0.1) × (6.35 ± 0.1); Temperature rise rate is 120 ℃/1h, and pressure is 1.82MPa, and setting deformation quantity is 0.21mm.
Differential scanning calorimeter (DSC) test.
The parts by weight composition of the raw material of embodiment 1-4 and comparative example 1,2 and material properties test data are as following table 1:
| Composition (weight part) | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
| PET | 100 | 100 | 100 | 100 | 100 | 100 |
| PBT | 20 | 28 | 35 | 40 | 35 | 35 |
| Mineral-filled thing | 10 | 20 | 30 | 40 | 30 | 30 |
| Toughner | 3 | 5 | 7 | 10 | 7 | 7 |
| Oxidation inhibitor | 0.3 | 0.4 | 0.5 | 0.6 | 0.5 | 0.5 |
| Processing aid | 0.2 | 0.3 | 0.5 | 0.6 | 0.5 | 0.5 |
| Heat-resistant agent | 0.5 | 0.7 | 1.0 | 1.2 | ||
| Nucleator | 0.5 | 0.6 | 0.8 | 1 | 0.8 | |
| Notched Izod impact strength (KJ/m2) | 7.2 | 8.0 | 8.4 | 8.7 | 7 | 9.5 |
| Tensile strength (MPa) | 53 | 57 | 62 | 63 | 48 | 55 |
| Elongation at break (%) | 3.2 | 5.3 | 6 | 6.4 | 3 | 6.5 |
| Flexural strength (MPa) | 82 | 84 | 94 | 95 | 73 | 90 |
| Modulus in flexure (MPa) | 2100 | 2300 | 2400 | 2660 | 1850 | 2330 |
| Heat-drawn wire (℃) | 120 | 135 | 140 | 142 | 105 | 132 |
Table 1
Composite material test DSC prepared by embodiment 3 schemes as shown in Figure 1, and composite material test DSC prepared by comparative example 2 schemes as shown in Figure 2, and composite material test DSC prepared by comparative example 1 schemes as shown in Figure 3.Analyze three DSC collection of illustrative plates, the material of comparative example 1 just starts to occur compared with large deformation under the environment of 125 degree, and the material of comparative example 2 occurs compared with large deformation under the environment of 185 degree, and the material of embodiment 3, under the environment of 205 degree, occurs compared with large deformation.By the deciphering to DSC collection of illustrative plates, PET/PBT matrix material prepared by the present invention can be worked under higher environment, and heat resistance is improved.By to embodiment 1-4 and the prepared matrix material of comparative example 1, carry out moulding, comparative analysis, the molded article of embodiment, surface gloss is much better than the molded article of comparative example 1.By to above analysis, the matrix material that the present invention is prepared has greatly improved compared with other general purpose materials in heatproof and surface gloss, has wide range of applications.
Above the embodiment of the present invention is described in detail, has applied specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof; , for one of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention meanwhile.
Claims (10)
1. high-temperature resistant high gloss PET/PBT matrix material, is characterized in that: by weight, composed of the following components:
2. high-temperature resistant high gloss PET/PBT matrix material according to claim 1, is characterized in that: the relative density of described PET is 1.35-1.38g/cm
3, fusing point is 250-260 ℃, the kinetic viscosity under molten state is 0.65-1.2 handkerchief second.
3. high-temperature resistant high gloss PET/PBT matrix material according to claim 1, is characterized in that: the relative density of described PBT is 1.30-1.34g/cm
3, fusing point is 222-227 ℃, the kinetic viscosity under molten state is 0.85-1.2 handkerchief second.
4. high-temperature resistant high gloss PET/PBT matrix material according to claim 1, is characterized in that: described mineral-filled thing is the polynary mineral-filled compound of self-control, and the preparation method of the polynary mineral-filled compound of described self-control is:
Silicates composite reinforcing fiber whisker, needle-like ground silica and process white are mixed by weight 1:0.5-0.6:0.5-0.6, separately add the nano silicon and the silane coupling agent that account for base-material gross weight 0.5%-2%, mix through high mixer, mixing temperature remains on 95 ℃, and mixing time is 30min.
5. high-temperature resistant high gloss PET/PBT matrix material according to claim 1, is characterized in that: described toughner is the one in EPDM grafted maleic anhydride or acrylic ester grafted Ethylene Propylene Terpolymer elastomerics.
6. high-temperature resistant high gloss PET/PBT matrix material according to claim 1, it is characterized in that: described oxidation inhibitor is four [3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and tricresyl phosphite (2,4-di-t-butyl phenyl ester) composite mixture or triglycol two-3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propylene is fine, one in three (2,4-di-tert-butylphenol) phosphorous acid ester.
7. high-temperature resistant high gloss PET/PBT matrix material according to claim 1, is characterized in that: described processing aid is the one in the modified product of OP wax, fatty acid or ethylene bis stearamide.
8. high-temperature resistant high gloss PET/PBT matrix material according to claim 1, it is characterized in that: described heat-resistant agent is triphenyl phosphite, Sodium Acid Pyrophosphate, ethyl sulfate one or several mixture of di (isooctyl) phosphate organic phosphoric acid compound.
9. high-temperature resistant high gloss PET/PBT matrix material according to claim 1, is characterized in that: described nucleator is mixed by one or several in long-chain line style saturated carboxylic acid sodium salt, long-chain line style saturated carboxylic acid calcium salt and aromatic carboxylic acid metal sodium salt or magnesium salts.
10. a preparation method for the high-temperature resistant high gloss PET/PBT matrix material as described in claim as arbitrary in claim 1-9, is characterized in that, comprises the following steps:
Step 1, take each component by parts by weight claimed in claim 1;
Step 2, by each component taking through high-speed mixing process 10-15 minute;
Step 3, by mixed step 2 material, melt extrude granulation through twin screw extruder; Twin screw extruder processing condition are: district's temperature is 190-230 ℃, and two district's temperature are 220-250 ℃, and three district's temperature are 230-265 ℃, and four district's temperature are 225-260 ℃, five district 230-265 ℃, and mixture is at spiral shell
In bar, time of delivery is 1-5min, and pressure is 10-18MPa.
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| CN105295314B (en) * | 2015-10-20 | 2019-02-05 | 上海胜南复合材料有限公司 | A kind of high-performance exempts from primary coat PBT/PET alloy material and preparation method |
| TWI705106B (en) * | 2018-12-25 | 2020-09-21 | 南亞塑膠工業股份有限公司 | High heat-resistant and high-gloss PBT composite material for vehicle lamp reflector and preparation method thereof |
| TWI711668B (en) * | 2019-01-30 | 2020-12-01 | 南亞塑膠工業股份有限公司 | Use of a low specific gravity PET composite material |
| CN112646332B (en) * | 2020-12-16 | 2023-04-14 | 上海金发科技发展有限公司 | Low-haze high-gloss PBT (polybutylene terephthalate) composite material and preparation method thereof |
| CN115895201A (en) * | 2022-10-14 | 2023-04-04 | 中广核瑞胜发（厦门）新材料有限公司 | High-reflectivity PBT composition suitable for manufacturing reflection cup and preparation and application thereof |
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| CN101974214A (en) * | 2010-09-29 | 2011-02-16 | 深圳市科聚新材料有限公司 | Mineral reinforced PC-PET composite material and preparation method thereof |
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